US4276019A - Process for regenerating of an adsorbing material in the form of particles charged with at least two volatile compounds having different thermal stabilities - Google Patents

Process for regenerating of an adsorbing material in the form of particles charged with at least two volatile compounds having different thermal stabilities Download PDF

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Publication number
US4276019A
US4276019A US06/089,370 US8937079A US4276019A US 4276019 A US4276019 A US 4276019A US 8937079 A US8937079 A US 8937079A US 4276019 A US4276019 A US 4276019A
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Prior art keywords
column
contacting
gas
inlet
suspension
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Expired - Lifetime
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US06/089,370
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English (en)
Inventor
Jean Remillieux
Albert Rebours
Philippe Dumortier
Paul H. L. Marchal
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PROCEDAIR SA
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Air Industrie SA
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Priority claimed from FR7830940A external-priority patent/FR2440222A1/fr
Priority claimed from FR7902941A external-priority patent/FR2447749A1/fr
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Publication of US4276019A publication Critical patent/US4276019A/en
Assigned to AIR INDUSTRIE ENVIRONMENT, A COMPANY reassignment AIR INDUSTRIE ENVIRONMENT, A COMPANY ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: AIR INDUSTRIE
Assigned to PROCEDAIR S.A. reassignment PROCEDAIR S.A. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: AIR INDUSTRIE ENVIRONNEMENT
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3458—Regenerating or reactivating using a particular desorbing compound or mixture in the gas phase
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/50—Aspects relating to the use of sorbent or filter aid materials
    • B01J2220/60—Use in several different columns
    • B01J2220/603—Use in several different columns serially disposed columns

Definitions

  • the present invention relates to a process for the regeneration of an adsorbent material in the form of particles charged with at least two volatile compounds having different thermal stabilities.
  • adsorbent materials for purifying smoke charged with harmful products before discharging this smoke into the atmosphere.
  • alumina is currently used, for example, for purifying the smoke from furnaces for baking anodes intended for electrolysis tanks, in the aluminium industry, this smoke containing particularly tars and compounds containing fluorine.
  • the problem is posed of regenerating the adsorbent particles charged with tars, compounds containing fluorine, or other harmful products, without the regeneration releasing these products, particularly the fluorine, into the atmosphere, and this while also removing the carbon dust which they may carry.
  • the compounds containing fluorine are heavily volatilized and a complementary purification of the air is provided to render it non-polluting for being discharged into the atmosphere.
  • the aim of the present invention is to provide a new process capable of resolving this problem of the regeneration of adsorbent particles, particularly of alumina, without the disadvantages of the known processes.
  • a process for the regeneration of an adsorbent material in the form of particles charged with at least two volatile compounds having different thermal stabilities is, in accordance with the invention, characterized in that calcination of one of said volatile compounds is caused in a first contacting column, in which said material is driven along and brought into suspension by an oxidizing gas stream, while being brought therein to a sufficiently high temperature, in that, at the outlet of said contacting column, a separation is effected between, on the one hand, said material, partially purified and, on the other hand, the driving gas and the gaseous products desorbed in the first column and in that, in a second contacting column, cooling of at least a part of said partially purified material is caused by bringing into suspension therein, while being driven along, in at least a part of the gases coming from the above-mentioned separation, these gases being cooled, so as to re-adsorb in this second column, on said material, said gaseous products desorbed in the first.
  • the gases from the second contacting column may be discharged into the atmosphere simply after conventional filtering, without it being necessary to provide an additional purifying installation, for example for removing the fluorine, in the case of the application mentioned above where the adsorbent material is charged with tars and compounds containing fluorine.
  • This fluorine is in effect re-adsorbed in said second column, having been desorbed in the first, and this without any additional consumption of alumina.
  • this material may also be provided for this material to be at least partially recycled at the inlet to said second column, to complete the re-adsorption, therein, of said gaseous products desorbed in the first column.
  • an oxidizing hopper with a porous bottom downstream of the separator which follows the first contacting column, oxygen or air being brought under this bottom to fluidize the material.
  • a process in accordance with the invention may further be characterized in that said oxidizing gas stream which, in the first contacting column, drives along and brings into suspension the adsorbent material to be generated, is formed by hot air whose temperature is regulated automatically depending on the measured temperature at the outlet of the columm, this air being possibly formed in part by new air, in part by recycling the already hot air obtained at the outlet of said first column after separation of the partially purified adsorbent material, the new air being moreover possibly pre-heated, in an exchanger, by taking heat from the part of the air directed towards the inlet of said second column.
  • This necessary cooling will moreover be increased by providing an input of new and fresh air, at a rate regulated automatically from a measurement of the temperature at the outlet of this column.
  • the size of the particles of adsorbent material may vary substantially, which also affects their heating-up rate: the result is that the distribution of temperatures along the calcination column may be affected thereby, overheating occuring either at the beginning of the distance covered, in the case of rapid combustion, or at the end of the distance covered, in the case of delayed combustion. This phenomenon may be accentuated by the presence, in more or less large proportions, of carbon-based dust, coming either from the smoke which the particles of alumina had served to purify, or more simply from a first stage of combustion of the tars.
  • the present invention aims further at avoiding such disadvantages and, at the same time improving the thermal efficiency of the process and, consequently, reducing the fuel costs.
  • the over-heating of the gases driving the material to be regenerated in the calcination column may be directly eliminated, as it occurs, along the calcination column, by means of an auxiliary gas stream flowing inside a double casing surrounding said column over at least a part of its length. It is thus possible to limit the temperature in this column so as to obtain an even temperature along the path of the flow of gas and adsorbing material.
  • This auxiliary gas current may be, here again, formed at least in part by new and fresh air which is then introduced, after being mixed with the recycled gases, into the inlet of said calcination column.
  • This stream of auxiliary gas contains an adjustable proportion of recycled hot gases coming from the calcination column.
  • auxiliary gas The general direction of the flow of auxiliary gas is chosen depending on the nature of the products which will be treated in the installation: --the same direction as that of the flow of material to be calcinated if its characteristics are likely to cause combustion of the major part of the polluting compounds at the beginning of the reaction; thus, the coldest auxiliary gas is in contact with the zone releasing most heat and the zone where the combustion is completed is not cooled excessively --in the opposite direction to that of the flow of material to be calcinated, if its characteristics are likely to cause a more progressive development of the reaction; thus, the coldest auxiliary gas is in contact with the most active combustion zone, and the zone for initiating the reaction is not cooled excessively.
  • the amount of new air introduced into the mixture which forms the flow of auxiliary cooling gas is regulated automatically and proportionally depending on the temperature of the gaseous current leaving the contacting column: since the cooling is precisely proportional to this amount of new air, it is thus possible, when the direction of flow of the stream of auxiliary gas is chosen as mentioned above, to stabilize perfectly the temperature of the column over the whole of its length.
  • the amount of heat to be absorbed by the cooling gas is proportional to the amount of pullutants to be burned: the amount of new air is then also proportional to this latter, which is an essential condition for good combustion.
  • FIG. 1 shows schematically a complete installation for implementing the invention
  • FIG. 2 is a partial schematic representation of an installation which may be of the same general type as the preceding one and used for the same purposes, but in which only the "calcination" part has been shown, including the calcination column and the means used for regulating the temperature in this column.
  • FIG. 1 shows an installation which will be assumed to be used for regenerating the alumina used for fixing by adsorption tars and compounds containing fluorine. It may be particularly alumina having served for purifying the smoke from furnaces for baking anodes for electrolysis tanks, for the production of aluminium. It will be understood that the aim of such an invention is then to rid the particles of alumina of the tars which they have adsorbed, without for all that allowing the fluorine to escape into the atmosphere.
  • the alumina to be treated is fed into a hopper with distributing screw 1, which brings the material, through a duct 2, downstream of the neck 3 of a venturi 4 for carrying out the suspension, which is effected by bringing hot air to the venturi through a pipe 5.
  • the hot air is produced by a gas re-heater 6.
  • the material brought into suspension is directed through a pipe 7 to the inlet of a first contacting column 8.
  • a sufficiently high temperature is maintained in this column to cause as complete a calcination as possible of the tars.
  • This temperature may be of the order of 450° to 900° C., the tars being calcined from about 450° C.
  • the temperature at the outlet of the column 8 is regulated.
  • a temperature sensor 9 is disposed on the outlet pipe 10 of the column, and whose signal, through a connection 11 and regulator 12, may control the opening of a valve 13 admitting combustible gas to the gas re-heater 6.
  • the gaseous part exits therefrom through a pipe 15 and the solid part through a distributing valve 14a.
  • a proportion of this gaseous part passing through pipe 15 may return to the inlet of contacting column 8 through a pipe 16, a suction device 17, the gas re-heater 6, pipe 5 and venturi 4.
  • the other part of this material is fed to the inlet of a second contacting column 20 for causing the re-adsorption, on the alumina, of the fluorine desorbed in the first column because of the presence therein of a high temperature.
  • the material may, here also, be put into suspension by bringing it downstream of the neck 21 of a venturi 22, in connection with said column 20 through a pipe 23.
  • the path of the powdery material between the distributing valve 18 and venturi 22 may be direct, but it may also comprise an oxidizing hopper 24 with a porous bottom 25, in which the material may be subjected to a complementary combustion for eliminating particularly the carbon which may remain sticking to the particles. For this, air or oxygen is introduced by a pipe 26 under the porous bottom 25.
  • Said path may also comprise a cooling device 27, shown with a dash-dot line in the figure and intended to lower the temperature of the particles.
  • this temperature in the second contacting column will be considerably lower than that which reigns in the first contacting column 8.
  • this temperature in the second contacting column will be less than 200° C.
  • venturi 22 For putting the particles of alumina in venturi 22 in suspension, it is possible to use as gas a part of the gases escaping from the separating device 14 through pipe 15 (the part of the gases which is not recycled through pipe 16 towards the inlet of venturi 4), the remaining part being formed by fresh air brought to venturi 22 through an inlet pipe 28 provided with a flow rate adjusting valve 29.
  • the pipe which brings it to the inlet of venturi 22. Since the particles at the outlet of separating device 14 may carry fine carbon and alumina dust (dust less than 15 microns), it may be advisable, so as not to find dust at the outlet of the installation, to provide in pipe 30 a filtering device 31. They could be conventional filters with filtering walls made of a woven material.
  • Pipe 30 may moreover, downstream of its connection with pipe 15 receiving gases from the separating device 14, be connected to an exchange element 30a of a heat exchanger whose other exchange element, shown at 32 in the figure, may connect the above-mentioned return pipe 16 to a source of new air with adjustable flow rate 33.
  • the hot gases coming from pipe 15 are cooled before being introduced through venturi 22 into the second contacting column 20 and, on the other hand, the new air of source 33 is re-heated before being fed, by suction device 17, into the first contacting column 8, through venturi 4.
  • the heat contained in the gases coming from separating device 14 is advantageously recovered.
  • the temperature in the second column 20 may be regulated by means of a temperature sensor 32 provided in its outlet pipe 35 and controlling, through a connection 36 and a regulator 37, the opening of the new air admission valve 29.
  • the temperature in the outlet pipe 35 may for example be fixed at 120° C.
  • the cooled powdery material on which the fluorine will have been re-adsorbed in contacting column 20 may be filtered in a filter 38 also conventional, the gaseous part thereof leaving through a pipe 39 before being discharged into the atmosphere by a fan 40, whereas the solid part is recovered at the bottom of a hopper 41 of the filter.
  • the alumina removed from the tar but having entirely re-adsorbed the fluorine desorbed in the first contacting column 8 may be removed through an outlet pipe 42, through a distributing valve 43, but from this latter a part of this material may also be recycled to venturi 22 through a pipe 44.
  • This arrangement enables the re-adsorption of the fluorine on the alumina to be completed and the determination of the proportion of the recycled part may be effected automatically, for example depending on a measurement of the fluorine content of the gases in discharge pipe 39.
  • the non-recycled portion of alumina coming from the outlet pipe 42 equal to the amount of alumina fed into the installation by hopper 1, it may be re-used for purifying smoke coming from the anode baking furnace, according to a known process.
  • Another portion of this alumina may also be used to supply the electrolysis tanks intended for the production of aluminium.
  • This may be particularly a chamber provided with burners, particularly gas burners, and in which a sheet of flame is formed which the powdery material in suspension will have to pass through before being introduced into the column. This is an arrangement which may be useful where there might be a risk of certain tar compositions not being entirely calcinated on leaving the column.
  • the separating device 14 may be formed by a single cyclone but may also and preferably comprise several small cyclones in parallel, these having a better separation efficiency.
  • the proportion of very fine particles in pipe 15 may be reduced and the clogging of the filtering device 31 delayed.
  • oxidizing hopper 24 is subjected to a slight depression so that the operation of the cyclone or cyclones of the separating device 14 is not disturbed.
  • This provision of a depression has been schematized in the drawing by a pipe 48 connected to any source of depression, for example at the inlet of suction device 17.
  • the hot air is, here also, produced by a gas heater 6 in which the fuel gas admission pipe is provided likewise with a flow rate adjusting valve 13, and the combustive air inlet pipe a blower 51 and a flow rate adjusting register 52.
  • the material brought into suspension is directed by duct 7 to the inlet of contacting column 8 which, here, is surrounded by a double casing 8a.
  • the space thus provided around column 8 may be given the shape of a helix by means of a helicoidal intermediate wall 8b.
  • the mixture coming from column 8 and formed of particles of alumina freed from tar, combustion gas, fluorine partially desorbed by the particles and air is, here also, fed by duct 10 to the separating device 14.
  • the gaseous part exits therefrom at S 1 through duct 15 and the solid part at S 2 through the distributing valve 14a.
  • this solid part exiting at S 2 may be subjected to a further treatment, for example cooling, with use, possibly, of the gaseous flow exiting at S 1 .
  • a certain proportion of the gaseous portion exiting through pipe 15 may return to the inlet of contacting column 8 through pipe 16, the suction device 17, the gas heater 6, pipe 5 and the device for putting the material into suspension 4.
  • the temperature at the outlet of column 8 is regulated to a standard value.
  • a temperature sensor 9 in outlet pipe 16 its signal, through the proportional acting regulator 12, may control in cascade, and successively, the valve 13 admitting combustible gas to gas heater 6 and register 49 adjusting the new and fresh air inlet 46.
  • regulator 12 controls first of all the reduction of the admission of combustible gas to heater 6 then, progressively, the opening of register 49 so as to admit a greater amount of new and fresh air.
  • the by-pass register 50 allows the proportion of gases from column 8 recycled by the heater to be adjusted without having previously circulated in the space of the double casing 8a.
  • the regulator 12 could control only the register 49 regulating the admission of new air 46, according to the procedure which has just been described.
  • the regulation of the input of combustible gas to heater 6 would then be achieved by means of a second regulator placed under the control of a temperature sensor which would be disposed in the inlet pipe 5 of the column.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
US06/089,370 1978-10-31 1979-10-30 Process for regenerating of an adsorbing material in the form of particles charged with at least two volatile compounds having different thermal stabilities Expired - Lifetime US4276019A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
FR7830940A FR2440222A1 (fr) 1978-10-31 1978-10-31 Procede de regeneration d'une matiere adsorbante se presentant sous forme de particules chargees d'au moins deux composes volatils de stabilites thermiques differentes
FR7830940 1978-10-31
FR7902941A FR2447749A1 (fr) 1979-02-05 1979-02-05 Procede de regeneration d'une matiere adsorbante se presentant sous forme de particules chargees d'un ou plusieurs composes organiques combustibles
FR7902941 1979-02-05

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US4276019A true US4276019A (en) 1981-06-30

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US06/089,370 Expired - Lifetime US4276019A (en) 1978-10-31 1979-10-30 Process for regenerating of an adsorbing material in the form of particles charged with at least two volatile compounds having different thermal stabilities

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US (1) US4276019A (fr)
EP (1) EP0011027B1 (fr)
AU (1) AU527328B2 (fr)
BR (1) BR7907051A (fr)
DE (1) DE2966675D1 (fr)
ES (1) ES8100096A1 (fr)
NO (1) NO152115C (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100381612C (zh) * 2006-11-28 2008-04-16 沈阳铝镁设计研究院 铝电解阳极焙烧炉烟气净化工艺及净化系统
CN105289202A (zh) * 2014-06-13 2016-02-03 贵阳铝镁设计研究院有限公司 一种沥青烟净化系统的加料方法及装置
US20170203976A1 (en) * 2016-01-19 2017-07-20 Mitsubishi Hitachi Power Systems Americas, Inc. Waste water evaporation methods and apparatus

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3904549A (en) * 1973-11-23 1975-09-09 Dorr Oliver Inc Fluidized bed regeneration of powdered activated carbon
US4174946A (en) * 1976-09-09 1979-11-20 Bergwerksverband Gmbh Process for drying coal in two-stage flow-through circulation heaters

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR748584A (fr) * 1932-01-08 1933-07-06 Procédé et appareil pour purifier et régénérer les matières siliceuses
FR1209223A (fr) * 1958-07-03 1960-02-29 Pechiney Procédé de récupération de gaz fluorhydrique par l'alumine
DE2127910C3 (de) * 1971-06-04 1984-08-02 Vereinigte Aluminium-Werke AG, 1000 Berlin und 5300 Bonn Verfahren zur thermischen Vergütung von Feststoffen, die aus Anlagen zur trockenen Reinigung von Abgasen aus Aluminiumelektrolyseöfen ausgetragen und zur Aluminiumelektrolyse als Einsatz verwendet werden

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3904549A (en) * 1973-11-23 1975-09-09 Dorr Oliver Inc Fluidized bed regeneration of powdered activated carbon
US4174946A (en) * 1976-09-09 1979-11-20 Bergwerksverband Gmbh Process for drying coal in two-stage flow-through circulation heaters

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100381612C (zh) * 2006-11-28 2008-04-16 沈阳铝镁设计研究院 铝电解阳极焙烧炉烟气净化工艺及净化系统
CN105289202A (zh) * 2014-06-13 2016-02-03 贵阳铝镁设计研究院有限公司 一种沥青烟净化系统的加料方法及装置
US20170203976A1 (en) * 2016-01-19 2017-07-20 Mitsubishi Hitachi Power Systems Americas, Inc. Waste water evaporation methods and apparatus
US11058967B2 (en) * 2016-01-19 2021-07-13 Mitsubishi Power Americas, Inc. Waste water evaporation methods and apparatus

Also Published As

Publication number Publication date
EP0011027A1 (fr) 1980-05-14
NO152115C (no) 1985-08-14
ES485501A0 (es) 1980-11-01
AU5226779A (en) 1981-04-07
AU527328B2 (en) 1983-02-24
NO152115B (no) 1985-04-29
NO793489L (no) 1980-05-02
EP0011027B1 (fr) 1984-02-15
BR7907051A (pt) 1980-07-15
DE2966675D1 (en) 1984-03-22
ES8100096A1 (es) 1980-11-01

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